HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-Chloro-6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran-4-ol | HCID 11009019 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-Chloro-6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran | HCID 53767658 | — |
Reaction Steps
To a solution of 6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran-4-ol (U.K. Patent Application GB 2 204 868A) (2.93 g) and triethylamine (4.04 ml) in dichloromethane (100 ml) was added methanesulphonylchloride (2.24 ml) over 30 min, under an atmosphere of nitrogen. The reaction mixture was stirred for 18 h, water was added and the organic phase separated, washed with aqueous sodium hydrogencarbonate and dried over anhydrous sodium sulphate. Filtration and evaporation of the solvent in vacuo gave the title compound (3.03g) as a solid, which was used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05053427 |
| Source dataset | uspto-grants-1991_10 |
| ORD ID | ord-4e17afd236b34c4b953cd66af90cdfe2 |
| Source note | uspto-grants-1991_10 |